CN1974407A - Production process of vanadium sesquioxide powder - Google Patents
Production process of vanadium sesquioxide powder Download PDFInfo
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- CN1974407A CN1974407A CN 200610022480 CN200610022480A CN1974407A CN 1974407 A CN1974407 A CN 1974407A CN 200610022480 CN200610022480 CN 200610022480 CN 200610022480 A CN200610022480 A CN 200610022480A CN 1974407 A CN1974407 A CN 1974407A
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Abstract
The present invention provides production process of vanadium sesquioxide powder with low reaction temperature and short reaction period. The production process includes the following steps: setting vanadium tetraoxide into one externally heated container; introducing reducing gas into the container; heating to 550-600 deg.c; maintaining the temperature to reduce for at least 3 min; and cooling to below 100 deg.c while isolating air and discharging to obtain the product. The process uses vanadium tetraoxide with relatively lower vanadium valence state as material, and has the advantages of simple reaction course, good reaction condition, low reductant consumption, high total vanadium yield, etc.
Description
Technical field
The invention belongs to chemical field, relate in particular to a kind of production method of vanadium sesquioxide powder.
Background technology
At present, the method for producing vanadous oxide generally adopts the direct-reduction process of additional reducing agent, produces by high temperature reduction.Used reductive agent comprises ammonia, hydrogen, carbon monoxide, methane or industrial gas etc.Produce that vanadous oxide is raw materials used Vanadium Pentoxide in FLAKES, ammonium meta-vanadate or ammonium poly-vanadate usually.CN94111901.7 discloses a kind of production method of vanadous oxide, and this method is that the ammonium vanadate of certain particle size or Vanadium Pentoxide in FLAKES are added in the external-heat container, and feeds industrial gas, and making the material decomposition-reduction is vanadous oxide.This method adopts common shaft furnace and rotary kiln as production unit, but the temperature height that this method requires in actual production (more than 900 ℃), high temperature material in the production unit is because the existence of some elements, the catalysis reason can influence the quality of subsequent product (as vanadium iron) because cause that C content increases in the product; In addition, the recovery time of this method is also long (in the actual production generally 30～40min).
Summary of the invention
Technical problem to be solved by this invention provides the production method of the vanadium sesquioxide powder that a kind of temperature of reaction is low, the reaction times is short.
The technical scheme that technical solution problem of the present invention is adopted is: the production method of vanadium sesquioxide powder, and this method may further comprise the steps: a) vanadium tetraoxide is joined in the outer heating container; B) reducing gas is passed in the container; C) be heated to 550～600 ℃; D) 3min is at least reduced in insulation; E) secluding air is cooled to come out of the stove below 100 ℃, obtains product.
Further, the described vanadium tetraoxide of step a is the powder vanadium tetraoxide, and size range is at 0.05mm～10.0mm.
Further, the material of the described container of step a is the alloy of steel or steel.
Further, the described container of step a is rotary kiln, fluidizing furnace, fluidized bed furnace, shaft furnace or multiple hearth furnace.
Further, the described reducing gas of step b is one or more of industrial gas, hydrogen or ammonia.
Further, when carrying out step b, keep pressure-fired in the container.
Further, the mode of the described heating of step c is an external heating mode.
Further, described external heating mode is gas-fired heating, combustion of natural gas heating, liquefied gas burning heating, gasoline combustion heating, kerosene burning heating, diesel combustion heating, microwave heating or electrically heated.
Further, the described refrigerative mode of step e is naturally cooling, forces cooling or carry out naturally cooling or the pressure cooling under protection of inert gas.
The invention has the beneficial effects as follows: the present invention adopts vanadium tetraoxide as raw material, because the valence state of vanadium is lower than raw material (ammonium vanadate, the Vanadium Pentoxide in FLAKES) valence state that traditional mode of production adopts in the raw material, reduction reaction is easier carries out, and reaction conditions is better, and the consumption of reductive agent can be lower.Therefore, temperature of reaction of the present invention is low, the reaction times short, and the vanadium sesquioxide powder that obtains contains vanadium can reach ∑ V=67.76%, and the rate of recovery of vanadium is more than 99.2%.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
The vanadium tetraoxide furnace charge is joined in the external-heating rotary kiln continuously, industrial gas and charging movement direction is reverse or feed in the same way in the rotary kiln, keep pressure-fired (10～20mmH in the kiln
2O), make by outer heating that the high temperature section temperature reaches 550 ℃ of scopes in the kiln, furnace charge fully contacts with coal gas, by gas reduction in this course at high temperature section residence time 8min.Subsequently furnace charge is cooled to kiln discharge below 100 ℃, obtains vanadium sesquioxide powder.
Vanadium sesquioxide powder ∑ V=66.84%, vanadium recovery 99.2%.
Embodiment 2:
The vanadium tetraoxide furnace charge is added in the fluidization boiler tube continuously from fluidized bed furnace boiler tube top, and the bottom feeding ammonia from the fluidized bed furnace boiler tube is heated to 600 ℃ with the fluidized bed furnace boiler tube simultaneously.Furnace charge is under the blowing of ammonia, and generation is seethed and flowed in the fluidized bed furnace boiler tube, cooling discharging mouth direction motion downwards, fully contact with ammonia in this course, reduced by ammonia, keep recovery time 5min in this temperature section insulation, furnace charge is reduced into vanadium sesquioxide powder.By bottom cooling discharging mouth, vanadium sesquioxide powder can be come out of the stove after being cooled to below 100 ℃ under the secluding air situation, obtain vanadium sesquioxide powder.
Vanadium sesquioxide powder ∑ V=67.65%, the rate of recovery 99.1% of vanadium.
Embodiment 3:
Add powder vanadium tetraoxide furnace charge in the shaft furnace continuously, hydrogen and charging movement direction is reverse or feed in the shaft furnace in the same way, make furnace high-temperature section temperature reach 570 ℃ of scopes by outer heating, furnace charge is at high temperature section residence time 5min, fully contact with hydrogen in this course, by hydrogen reducing.Enter cooling section subsequently, furnace charge is cooled to come out of the stove below 100 ℃, obtain vanadium sesquioxide powder.
Vanadium sesquioxide powder ∑ V=67.76, vanadium recovery 99.3%.
Claims (9)
1, the production method of vanadium sesquioxide powder is characterized in that, this method may further comprise the steps:
A) vanadium tetraoxide is joined in the outer heating container;
B) reducing gas is passed in the container;
C) be heated to 550～600 ℃;
D) 3min is at least reduced in insulation;
E) secluding air is cooled to come out of the stove below 100 ℃, obtains product.
2, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the described vanadium tetraoxide of step a is the powder vanadium tetraoxide, and size range is at 0.05mm～10.0mm.
3, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the material of the described container of step a is the alloy of steel or steel.
4, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the described container of step a is rotary kiln, fluidizing furnace, fluidized bed furnace, shaft furnace or multiple hearth furnace.
5, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the described reducing gas of step b is one or more of industrial gas, hydrogen or ammonia.
6, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: when carrying out step b, keep pressure-fired in the container.
7, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the mode of the described heating of step c is an external heating mode.
8, the production method of vanadium sesquioxide powder according to claim 7 is characterized in that: described external heating mode is gas-fired heating, combustion of natural gas heating, liquefied gas burning heating, gasoline combustion heating, kerosene burning heating, diesel combustion heating, microwave heating or electrically heated.
9, the production method of vanadium sesquioxide powder according to claim 1 is characterized in that: the described refrigerative mode of step e is naturally cooling, forces cooling or carry out naturally cooling or the pressure cooling under protection of inert gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100224807A CN100457635C (en) | 2006-12-12 | 2006-12-12 | Production process of vanadium sesquioxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100224807A CN100457635C (en) | 2006-12-12 | 2006-12-12 | Production process of vanadium sesquioxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1974407A true CN1974407A (en) | 2007-06-06 |
| CN100457635C CN100457635C (en) | 2009-02-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100224807A Expired - Fee Related CN100457635C (en) | 2006-12-12 | 2006-12-12 | Production process of vanadium sesquioxide powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708554A (en) * | 2014-01-16 | 2014-04-09 | 江苏理工学院 | Method for preparing vanadium trioxide nanosphere |
| CN104118910A (en) * | 2014-06-24 | 2014-10-29 | 中国科学院过程工程研究所 | Method for selectively preparing vanadium oxides and recovering hydroxides through vanadate hydrogen reduction method |
| CN106006734A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using vanadium-containing solution for preparing vanadium trioxide |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN108423712A (en) * | 2018-04-12 | 2018-08-21 | 四川星明能源环保科技有限公司 | Vanadium trioxide and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052460C (en) * | 1994-09-15 | 2000-05-17 | 攀枝花钢铁(集团)公司 | Method for producing V2O3 |
-
2006
- 2006-12-12 CN CNB2006100224807A patent/CN100457635C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708554A (en) * | 2014-01-16 | 2014-04-09 | 江苏理工学院 | Method for preparing vanadium trioxide nanosphere |
| CN103708554B (en) * | 2014-01-16 | 2015-05-20 | 江苏理工学院 | Method for preparing vanadium trioxide nanosphere |
| CN104118910A (en) * | 2014-06-24 | 2014-10-29 | 中国科学院过程工程研究所 | Method for selectively preparing vanadium oxides and recovering hydroxides through vanadate hydrogen reduction method |
| CN106006734A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using vanadium-containing solution for preparing vanadium trioxide |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN108423712A (en) * | 2018-04-12 | 2018-08-21 | 四川星明能源环保科技有限公司 | Vanadium trioxide and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100457635C (en) | 2009-02-04 |
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Granted publication date: 20090204 Termination date: 20091212 |